CN106800291A - A kind of preparation method of Graphene - Google Patents
A kind of preparation method of Graphene Download PDFInfo
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- CN106800291A CN106800291A CN201510832035.6A CN201510832035A CN106800291A CN 106800291 A CN106800291 A CN 106800291A CN 201510832035 A CN201510832035 A CN 201510832035A CN 106800291 A CN106800291 A CN 106800291A
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Abstract
The present invention discloses a kind of preparation method of Graphene, and the preparation method of the Graphene comprises the following steps：By pyridine and formic acid according to volume ratio 1:1‑1:5 ratio is well mixed, and obtains mixed solvent；Graphite oxide is scattered in the mixed solvent, mixed solution is obtained, the graphite oxide is 5 7mg/ml with the adding proportion of the mixed solvent；The mixed solution is carried out into the 40min of ultrasonic disperse 30；The addition 0.5ml of methyl-silicone oil 0.2, carries out atmospheric pressure reflux reaction, until atrament is no longer separated out, stops back flow reaction；By product separating-purifying, pretreating graphite alkene is obtained；Pretreating graphite alkene is coated on substrate；Substrate to being provided with pretreating graphite alkene carries out laser reduction, obtains Graphene finished product.The preparation method of the Graphene that the present invention is provided, by selecting rational reducing agent and related process parameters, is reduced sufficiently graphite oxide, not only increases its reducing degree, and improve the product quality of Graphene.
Description
Technical field
The present invention relates to graphite technology field, and in particular to a kind of preparation method of Graphene.
Background technology
Used as a kind of carbon material of new bi-dimensional cellular shape structure, it has good electric conductivity to Graphene（7200 S/m）, larger theoretical specific surface area (2600 m2/ g), the superior performance such as high mechanical stability, therefore cause extensive concern.The method for preparing Graphene at present mainly has：（1）Graceful Chester university An Deli of micromechanics stripping method, such as Britain et al. prepares Graphene using adhesive tape method, though the method can obtain quality few layer graphene higher, yield is relatively low, process is cumbersome limits it and use；（2）Chemical vapour deposition technique, the method be in the reactor with catalyst substrate, carbon atom on substrate deposition growing into Graphene, the method can produce substantial amounts of Graphene, but the growth conditions of Graphene is harsh, cost is also higher.（3）Oxidation-reduction method, the method includes two steps：Graphite aoxidizes to form graphite oxide through strong oxidizer, and graphite oxide obtains Graphene through chemistry or thermal reduction.It is widely used because the method cost is relatively low, simple to operate.
Chemical reduction method is considered as the effective ways for largely preparing Graphene, and conventional reducing agent has hydrazine hydrate, hydroquinones etc., but these reducing agents high toxicity, have greatly harm to environment and human body.Therefore new hypotoxicity reducing agent gradually attracts attention.However, the reaction condition of prior art makes hypotoxicity reducing agent in preparation technology, Graphene can produce a large amount of reunions, and agglomeration reduces the reducing degree of graphite oxide, influences the product quality of Graphene.
Therefore, it is necessary to provide a kind of preparation method of graphite oxide reducing degree Graphene high.
The content of the invention
The purpose of the present invention is to overcome above-mentioned technical problem, there is provided a kind of graphite oxide reducing degree is high, the preparation method of the measured Graphene of graphene product matter.
In order to solve the above technical problems, the preparation method of the Graphene that the present invention is provided, comprises the following steps：
S1：By pyridine and formic acid according to volume ratio 1:1-1:5 ratio is well mixed, and obtains mixed solvent；
S2：Graphite oxide is scattered in the mixed solvent, mixed solution is obtained, the graphite oxide is 5-7mg/ml with the adding proportion of the mixed solvent；
S3：The mixed solution is carried out into ultrasonic disperse 30-40min；
S4：Addition methyl-silicone oil 0.2-0.5ml, carries out atmospheric pressure reflux reaction, until atrament is no longer separated out, stops back flow reaction；
S5：By product separating-purifying, pretreating graphite alkene is obtained；
S6：Pretreating graphite alkene is coated on substrate；
S7：Substrate to being provided with pretreating graphite alkene carries out laser reduction, obtains Graphene finished product.
Preferably, in the step S1, the mixing ratio of the pyridine and the formic acid is 1:4.
Preferably, in the step S2, the graphite oxide is 5mg/ml with the adding proportion of the mixed solvent.
Preferably, in the step S4, the addition of the methyl-silicone oil is 0.2ml.
Preferably, in the step S6, the substrate is aluminium foil or silicon chip.
Compared with prior art, the preparation method of the Graphene that the present invention is provided, by selecting rational reducing agent and related process parameters, is reduced sufficiently graphite oxide, not only increases its reducing degree, and improve the product quality of Graphene.
Specific embodiment
Below in conjunction with implementation method, the invention will be further described.
Embodiment 1
Embodiment 1
A kind of preparation method of Graphene, comprises the following steps：
S1：By pyridine and formic acid according to volume ratio 1:4 ratio is well mixed, and obtains mixed solvent；
S2：Graphite oxide is scattered in the mixed solvent, mixed solution is obtained, the graphite oxide is 5mg/ml with the adding proportion of the mixed solvent；
S3：The mixed solution is carried out into ultrasonic disperse 30min；
S4：Addition methyl-silicone oil 0.2ml, carries out atmospheric pressure reflux reaction, until atrament is no longer separated out, stops back flow reaction；
S5：By product separating-purifying, pretreating graphite alkene is obtained；
S6：Pretreating graphite alkene is coated on substrate, the substrate is aluminium foil；
S7：Substrate to being provided with pretreating graphite alkene carries out laser reduction, obtains Graphene finished product.
Embodiment 2
A kind of preparation method of Graphene, comprises the following steps：
S1：By pyridine and formic acid according to volume ratio 1:5 ratio is well mixed, and obtains mixed solvent；
S2：Graphite oxide is scattered in the mixed solvent, mixed solution is obtained, the graphite oxide is 7mg/ml with the adding proportion of the mixed solvent；
S3：The mixed solution is carried out into ultrasonic disperse 40min；
S4：Addition methyl-silicone oil 0.3ml, carries out atmospheric pressure reflux reaction, until atrament is no longer separated out, stops back flow reaction；
S5：By product separating-purifying, pretreating graphite alkene is obtained；
S6：Pretreating graphite alkene is coated on substrate, the substrate is silicon chip；
S7：Substrate to being provided with pretreating graphite alkene carries out laser reduction, obtains Graphene finished product.
Embodiment 3
A kind of preparation method of Graphene, comprises the following steps：
S1：By pyridine and formic acid according to volume ratio 1:1 ratio is well mixed, and obtains mixed solvent；
S2：Graphite oxide is scattered in the mixed solvent, mixed solution is obtained, the graphite oxide is 6mg/ml with the adding proportion of the mixed solvent；
S3：The mixed solution is carried out into ultrasonic disperse 35min；
S4：Addition methyl-silicone oil 0.5ml, carries out atmospheric pressure reflux reaction, until atrament is no longer separated out, stops back flow reaction；
S5：By product separating-purifying, pretreating graphite alkene is obtained；
S6：Pretreating graphite alkene is coated on substrate, the substrate is aluminium foil；
S7：Substrate to being provided with pretreating graphite alkene carries out laser reduction, obtains Graphene finished product.
The preparation method of the Graphene that the present invention is provided, by selecting rational reducing agent and related process parameters, is reduced sufficiently graphite oxide, not only increases its reducing degree, and improve the product quality of Graphene.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the invention is limited; equivalent structure or equivalent flow conversion that every utilization present specification is made; or other related technical fields are directly or indirectly used in, it is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of Graphene, it is characterised in that comprise the following steps：
S1：By pyridine and formic acid according to volume ratio 1:1-1:5 ratio is well mixed, and obtains mixed solvent；
S2：Graphite oxide is scattered in the mixed solvent, mixed solution is obtained, the graphite oxide is 5-7mg/ml with the adding proportion of the mixed solvent；
S3：The mixed solution is carried out into ultrasonic disperse 30-40min；
S4：Addition methyl-silicone oil 0.2-0.5ml, carries out atmospheric pressure reflux reaction, until atrament is no longer separated out, stops back flow reaction；
S5：By product separating-purifying, pretreating graphite alkene is obtained；
S6：Pretreating graphite alkene is coated on substrate；
S7：Substrate to being provided with pretreating graphite alkene carries out laser reduction, obtains Graphene finished product.
2. the preparation method of Graphene according to claim 1, it is characterised in that in the step S1, the mixing ratio of the pyridine and the formic acid is 1:4.
3. the preparation method of Graphene according to claim 1, it is characterised in that in the step S2, the graphite oxide is 5mg/ml with the adding proportion of the mixed solvent.
4. the preparation method of Graphene according to claim 1, it is characterised in that in the step S4, the addition of the methyl-silicone oil is 0.2ml.
5. the preparation method of Graphene according to claim 1, it is characterised in that in the step S6, the substrate is aluminium foil or silicon chip.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311153A (en) * | 2016-04-25 | 2017-11-03 | 湖南国盛石墨科技有限公司 | A kind of preparation method of graphene |
| CN107445151A (en) * | 2017-09-07 | 2017-12-08 | 南京汉尔斯生物科技有限公司 | Graphene, Graphene electrodes and preparation method thereof |
| CN110723725A (en) * | 2019-11-04 | 2020-01-24 | 中国科学院福建物质结构研究所 | Low-power laser reduction graphene film and preparation method thereof |
| CN110723726A (en) * | 2019-11-04 | 2020-01-24 | 中国科学院福建物质结构研究所 | Laser reduction graphene film and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765716A (en) * | 2012-07-17 | 2012-11-07 | 上海大学 | Preparation method of graphene |
| CN103508447A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN104211047A (en) * | 2013-05-30 | 2014-12-17 | 纳米新能源（唐山）有限责任公司 | Graphene, graphene electrode, graphene supercapacitor and preparation method thereof |
-
2015
- 2015-11-25 CN CN201510832035.6A patent/CN106800291A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508447A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN102765716A (en) * | 2012-07-17 | 2012-11-07 | 上海大学 | Preparation method of graphene |
| CN104211047A (en) * | 2013-05-30 | 2014-12-17 | 纳米新能源（唐山）有限责任公司 | Graphene, graphene electrode, graphene supercapacitor and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311153A (en) * | 2016-04-25 | 2017-11-03 | 湖南国盛石墨科技有限公司 | A kind of preparation method of graphene |
| CN107445151A (en) * | 2017-09-07 | 2017-12-08 | 南京汉尔斯生物科技有限公司 | Graphene, Graphene electrodes and preparation method thereof |
| CN110723725A (en) * | 2019-11-04 | 2020-01-24 | 中国科学院福建物质结构研究所 | Low-power laser reduction graphene film and preparation method thereof |
| CN110723726A (en) * | 2019-11-04 | 2020-01-24 | 中国科学院福建物质结构研究所 | Laser reduction graphene film and preparation method thereof |
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Application publication date: 20170606 |